Hydrazine hydrate (1:1) → HCID 135519368、化合物

HRID 1296956ノート

反応式

HRID 1296956 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[OH:12])[O:8][C:7]([C:13]([OH:15])=[O:14])=[C:6]([C:16]1[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=1)[C:5]2=O.O.[NH2:26][NH2:27]>C(O)C.C([O-])(O)=O.[Na+]>[Cl:1][C:2]1[C:11]([OH:12])=[CH:10][C:9]([OH:8])=[C:4]([C:5]2[C:6]([C:16]3[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=3)=[C:7]([C:13]([OH:15])=[O:14])[NH:26][N:27]=2)[CH:3]=1

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 11416722HCID 11416722、化合物

生成物 1

HCID 135519368HCID 135519368、化合物

試薬・触媒・溶媒 2

HCID 516892Sodium Bicarbonate触媒HCID 702Ethanol溶媒

反応条件

温度
70 °C

実験手順

6-Chloro-7-hydroxy-3-(4-methoxy-phenyl)-4-oxo-4H-chromene-2-carboxylic acid (1 eq) was taken up in ethanol and hydrazine hydrate (3 eq) was added. To aid dissolution a few drops of NaHCO3 (aq) was added, and then all was heated at 70° C. under nitrogen for 2 hours. The solution was cooled to room temperature and concentrated in vacuo to a brown oil. This was partitioned between 1M HCl (aq) and diethyl ether. The organic phases were combined, washed with 1M HCl (aq), dried over MgSO4, filtered and concentrated in vacuo to give 5-(5-chloro-2,4-dihydroxy-phenyl)-4-(4-methoxy-phenyl)-2H-pyrazole-3-carboxylic acid as a yellow foam.

後処理

  1. additionwas added
  2. temperatureThe solution was cooled to room temperature
  3. concentrationconcentrated in vacuo to a brown oil
  4. customThis was partitioned between 1M HCl (aq) and diethyl ether
  5. washwashed with 1M HCl (aq)
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-98a05657a50a4ebb8193f511c258c0f6
出典データセット
uspto-grants-2007_07
特許番号
US07247734B2

反応ノート

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